Reaktion #742267

Reaktionsgleichung

acetonitrile

1-bromo-2-[(2-bromoethyl)-disulphanyl]ethane

N-methylpyrrolidone

2-picoline

→

light beige product

1,1′-(disulphanediyldiethane-2,1-diyl)bis(2-methylpyridinium)dibromide

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGThe mixture (white suspension) is kept stirring at 80° C. for 30 min
2. 2
   Temperaturthe stirring is maintained at 80° C. for 90 min
3. 3
   TemperaturAfter cooling
4. 4
   Sonstigethe solid obtained
5. 5
   Filtrationis filtered off
6. 6
   Waschenwashed with 100 ml of ACN
7. 7
   Sonstigedried
8. 8
   Sonstige56.2 g of brown powder are recovered
9. 9
   Temperaturat reflux
10. 10
    workup.ADDITIONOnce the temperature has dropped to 40° C.
11. 11
    Filtrationthe solid is filtered off
12. 12
    Waschenwashed with 3 times 100 ml of iPrOH
13. 13
    Sonstigedried under vacuum

Vorschrift

A mixture of 56 g of 1-bromo-2-[(2-bromoethyl)-disulphanyl]ethane and 15 ml of N-methylpyrrolidone (NMP) is poured dropwise onto 35 g of 2-picoline with stirring, at 80° C. The mixture (white suspension) is kept stirring at 80° C. for 30 min, 100 ml of acetonitrile (ACN) are added, and the stirring is maintained at 80° C. for 90 min. After cooling, the solid obtained is filtered off, washed with 100 ml of ACN and then dried. 56.2 g of brown powder are recovered. 45 g of this powder are suspended in 300 ml of isopropanol (iPrOH), at reflux. Once the temperature has dropped to 40° C., the solid is filtered off, washed with 3 times 100 ml of iPrOH and dried under vacuum. 40.56 g of a light beige product are obtained. The analyses are in conformity with the expected structure.

Quelle